反应详情

温度

0 °C

To a 0° C. solution of 0.674 g 2-(aminomethyl)pyridine, 20 ml methylene chloride and 1.83 ml pyridine is added, dropwise over 20 minutes, 2.0 g of product from Example 3 dissolved in 25 ml of methylene chloride. The reaction is stirred at 0° C. for 2 hours followed by stirring at room temperature for 17 hours. The reaction mixture is partitioned between chloroform and saturated sodium bicarbonate, washed with water and saturated sodium chloride, dried and concentrated in vacuo. The residue is purified by column chromatography (silica gel:75% ethyl acetate/hexane) to give 1.51 g of the desired product.

1. stirringby stirring at room temperature for 17 hours
2. customThe reaction mixture is partitioned between chloroform and saturated sodium bicarbonate
3. washwashed with water and saturated sodium chloride
4. customdried
5. concentrationconcentrated in vacuo
6. customThe residue is purified by column chromatography (silica gel:75% ethyl acetate/hexane)